201111282 六、發明說明： 【發明所屬之技術領域】 本發明係關於負/卜4E h 2 ^ . 虱化鎂粒子、其製造方法、散熱性填料、 樹脂組成物、散熱性潤滑脂及散熱性塗料組成物。 【先前技術】 氧化鎮係耐熱性、導熱性、電絕緣性優異之化合物， 且廣泛使用於橡膠之硫化促進劑；塗料、油墨用顏料·醫 樂品各種產業領域。作為此種氧化鎂之各種用途之一，提 出有散熱性填料。（專利文獻1等）。 作為此種散熱性填料，廣泛使用氧化紹或氣化紹等。 然而，氧化鋁之莫氏硬度高，在散熱片等之製造過程中， 有混練機磨耗嚴重之缺點。又，氮化鋁之填充性較差，有 難以於樹脂令進行高填充之缺點。又，氮化結價格高，亦 有散熱構件變得價格高之缺點。因此，需要與該等原料不 同之新散熱性填料。 另一方面，因氧化鎂粒子為莫氏硬度低、比重輕之化 5物故有操作性優異之優點。進而，其係電阻值較高之 素材，因此亦適用於電氣、電子領域。然而，作為散熱性 填料使用時，必須可於形成成形物之樹脂中進行高填充。 因此，需要粒子之凝聚狀態或粒徑分佈獲得控制之氧化 鎂。但是，於專利文獻1中，記載有控制一次粒徑，但關 於粒子之凝聚比例或粒子分佈獲得控制之粒子並未記載。 又，於散熱性填料以外之如上所述之各種氧化鎂之用 途中’亦期待藉由使用具有特異性粒度分佈之氧化鎂，而 201111282 發揮與先前不同之物性之新效果。 t文獻1 :日本特開2009一7215號公報 【發明内容】 本發明之目的在於楹 散埶k七、—種比先前之氧化鎂更適用於 填枓專之用途的氧化鎮粒子。 本發明之氧化鎂粒 面積求得之比表面積:):比tr在於:(中徑)取表 上述氧化鎮粒子，=為為3；7，D90/Dl0為4以下。 於1_〜1崎锻燒氨氧化鎮而得。U在下， 亡=匕鎮粒子’較佳為，藉由相對 莫耳以合以观換算為 煅燒而得。 10莫耳份之硼酸或其鹽，進行 上述删酸或其雎，如从& 物、四十水V、：:二由四…—五水合 錢-四水合物所組成之群中之至：―種四水合物及四賴 上述氧化鎂粒子，較佳為 得。 艰步進仃表面處理而 本發明係上述氧化鎮粒子之製 具有於硼酸或其踏存彳Τ 方法，其特徵在於： 之步I 4在下’於咖〜i_t：㈣氫氧化鎮 上述氧化鎂粒子之製造方法 氧化鎂100莫耳份.、f人、， 佳為具有相對於氫 合以算為G」〜 其鹽，進行煅燒之步驟。 莫平仏之硼酸或 上述硼酸或其鹽，較 為選自由四硼酸鋰五水合 201111282 物、，鈉〜十水合物、四 銨一四水合物赂,α 四水合物及四硼酸 物所組成之群中之至少一種。 本發明亦為一種散熱,f生填料，其特 化鎂粒子構成。 仕π·由上述氧 本發明亦為一種樹脂組成物，其 氧化鎂粒子。 牧γ 3有上述 本發明亦為一種散熱性潤滑脂，其特徵在於 逆氣化鎮粒子。 、 3有上 亦為一種散熱性塗料組成物， 有上述氧化鎂粒子。 ^ 3 本發明之氧化鎂粒子，因粒度分佈陡 程度得到控制，故可對 粒子之凝聚 此’可作為優異 丁问填充。藉 雯兵之散熱性材料使用。又， 之硫化促進劑：塗 冑用於橡膠 【實施方式】 肖顏抖，邊樂品等領域中。 以下，詳細說明本發明。 本發明之氧化鎂粒子之特徵在於：（ 積求得之比表面積徑（以下，表示為似徑）=比表面 D90/D10為4以下。 為3以下， 於使用乳化鎮粒子作為散熱材之情形時 散熱性，而期望撻古鈿士、* 马了獲得尚 中之粒子填充率。為了獲得-充羊’重要的是控制凝聚狀態或。： 獲得以高水準控制凝聚狀態或形狀之氧化^此，要求 了達成此種目的，滿足如 、。發現為 乩〈符疋參數之粗子良好， 201111282 藉此完成本發明。 進而，如上所述之粒徑或形狀得到控制之氧化鎮’若 組合，用複數個粒徑不同者，則於可獲得更高之填充率、 可獲得優異之散熱性能方面亦較佳。 本發明之氧化鎮粒子係粒子之凝聚度與粒徑分佈得到 控制者。（中徑）/(SSA徑）之比A矣_』^ ;之比為表不粒子之凝聚度之值。 中把為反映二次粒徑之粒經，似徑為反映一次粒徑之粒 因此’上述比成為表示構成二次粒子之一次粒子的數 里之參數。本發明之氣^卜赵4 2 货乃之乳化鎮拉子係具有相對較少之數量的201111282 VI. Description of the Invention: [Technical Field] The present invention relates to negative/b 4E h 2 ^ . Magnesium telluride particles, a method for producing the same, a heat-dissipating filler, a resin composition, a heat-dissipating grease, and a heat-dissipating paint Composition. [Prior Art] Oxidizing towns are excellent in heat resistance, thermal conductivity, and electrical insulating properties, and are widely used in rubber vulcanization accelerators; paints, inks, and medical products. As one of various uses of such magnesium oxide, a heat-releasing filler has been proposed. (Patent Document 1, etc.). As such a heat-dissipating filler, oxidized or gasified is widely used. However, the Mohs hardness of alumina is high, and there is a disadvantage that the kneading machine is severely worn during the manufacturing process of the heat sink or the like. Further, the filling property of aluminum nitride is inferior, and it is difficult to achieve high filling of the resin. Further, the price of the nitrided joint is high, and there is also a disadvantage that the heat radiating member becomes expensive. Therefore, new heat-dissipating fillers are required that are different from these materials. On the other hand, since the magnesium oxide particles have a low Mohs hardness and a light specific gravity, they are excellent in handleability. Further, it is a material having a high resistance value, and is therefore also suitable for use in the electrical and electronic fields. However, when used as a heat-dissipating filler, it is necessary to perform high filling in the resin forming the molded article. Therefore, it is necessary to obtain controlled magnesium oxide in the state of aggregation or particle size distribution of the particles. However, Patent Document 1 describes that the primary particle diameter is controlled, but the particles which are controlled by the aggregation ratio of the particles or the particle distribution are not described. Further, in the case of using various kinds of magnesium oxide as described above other than the heat-dissipating filler, it is expected to use a magnesium oxide having a specific particle size distribution, and 201111282 exerts a new effect different from the previous physical properties. t Document 1: Japanese Laid-Open Patent Publication No. 2009-7215 SUMMARY OF THE INVENTION The object of the present invention is to provide an oxidized town particle which is more suitable for filling purposes than the prior magnesium oxide. The specific surface area obtained by the area of the magnesium oxide particles of the present invention:): The ratio tr is: (medium diameter) is taken as the above-mentioned oxidized town particles, = 3; 7 and D90/D10 are 4 or less. It is obtained from 1_~1 Saki forging ammonia oxidation town. U is lower, and the granules of 亡 = 匕 are preferably obtained by calcination with respect to the molars. 10 moles of boric acid or a salt thereof, which is subjected to the above-mentioned acid scavenging or its hydrazine, such as from the group consisting of & matter, forty water V, :: two from four...-pentahydrate-tetrahydrate : A seed tetrahydrate and the above-mentioned magnesium oxide particles are preferably obtained. The invention is characterized in that the above-mentioned oxidized granules are produced by boric acid or a method thereof, which is characterized in that: step I 4 is in the lower of the above-mentioned magnesium oxide particles of yoghurt~i_t: (d) The production method is a step of calcining 100 parts of magnesium oxide, f, and preferably having a G" to a salt thereof with respect to hydrogen. The boric acid of moping or the above boric acid or a salt thereof is selected from the group consisting of lithium tetraborate pentahydrate 201111282, sodium to decahydrate, tetraammonium tetrahydrate, alpha tetrahydrate and tetraborate. At least one of them. The invention is also a heat dissipating, f-grown filler composed of specialized magnesium particles. The present invention is also a resin composition of magnesium oxide particles. The present invention is also a heat-dissipating grease characterized by inverse gasification of the particles. And 3 is also a heat-dissipating paint composition having the above-mentioned magnesium oxide particles. ^ 3 The magnesium oxide particles of the present invention are controlled by the steepness of the particle size distribution, so that the aggregation of the particles can be used as an excellent filling. Use the heat-dissipating material of Wen Bing. Further, the vulcanization accelerator: coated with ruthenium for rubber [Embodiment] Xiao Yan shake, side music and other fields. Hereinafter, the present invention will be described in detail. The magnesium oxide particles of the present invention are characterized in that the specific surface area diameter (hereinafter referred to as the diameter) is 4 or less than the surface D90/D10. It is 3 or less, and the emulsified town particles are used as the heat dissipation material. At the time of heat dissipation, it is expected that the ancient gentleman and the horse will obtain the particle filling rate of the Shangzhong. In order to obtain the -filled sheep, it is important to control the condensed state or to obtain the oxidation of the condensed state or shape at a high level. It is required to achieve such a goal, satisfying the conclusion that the roughness of the parameter is good, and 201111282, thereby completing the present invention. Further, as described above, the particle size or shape is controlled by the oxidation town. It is also preferable to obtain a higher filling ratio and obtain excellent heat dissipation performance by using a plurality of different particle diameters. The degree of aggregation and particle size distribution of the oxidized particles of the present invention are controlled. The ratio of the diameter)/(SSA diameter) to A矣_』^; is the value of the degree of aggregation of the particles. The medium is the particle that reflects the secondary particle size, and the diameter is the particle that reflects the primary particle size. The above ratio becomes the representation The parameter of the number of primary particles of the secondary particles. The emulsified Zhenla series of the gas of the present invention has a relatively small number of
-人粒子凝聚而形成之--U 丄“ 仏成之…人粒子者。此種粒子在於樹脂或 油專中之分散性優異之方面較為有利，特別適於散熱材料。 本發明之氧化鎮粒子係上述中徑/SSA徑達到3以下 者，更佳為2.8以下’再更佳為27以下。 、進而，本發明之氧化鎂粒子之特徵在於：因D90/D10 為4以下，故其粒徑分佈陡靖。若為此種粒徑分佈陡崎之 粒子，則容易控制填充率’因此於可容易地獲得具有高散 熱性之組成物方面較佳。上述〇9〇/〇1〇更佳為39以下。 贫即’本發明之氧化鎂粒子之特徵在於··數量少於先前 之氧化鎖粒子之一次粒子凝聚而形成二次粒子，且D90與 之比j (即，粒從之分佈為陡峭卜此種氧化鎂粒子並非 眾所周知，係由本發明者等人首次製造。 上述中控亦稱為D5〇’係指在將粉體根據某一粒徑分成 種夺較大者與較小者為等量之徑。於D ^ 同樣地 測定粒徑分佈之情形時，將較小者㈣1〇%之粒徑稱為 201111282 DW，將較小者達到90%之粒徑稱為奶〇。dm、^ 係分別藉由測定粒徑分佈而獲得之值，於本發明巾，、：: 分佈係藉由雷射繞射粒度分佈測 立值 司製Mic贈ac M丁 33〇〇 Εχ)所挪得之值。股伤有限公 常之ΐΐΠ徑係基於以下前提所求得之值：根據藉由通 承之方法所測定之ΒΕΤ比表面積，粒子為圓球。 上述氧化鎂粒子對粒徑並無特 热符別限疋，但令徑較佳為 〇· 1〜25 # m，下限更佳為1 V m即，如上所述之範圍廣 泛之粒徑範圍内之氧化鎂粒子 J用作散熱材，且可製成蒋 得高填充率所需之任意大小者。 展成獲 上述氧化鎂粒子對粒徑並無 业热特別限疋，但SSA徑較佳 馬U.1〜15#m，下限更佳為 尺住马1 “ 即，如上所述之範圍 廣泛之粒徑範圍内之邀#赶& ^ η η 氧化鎮拉子可用作散熱材，且可製成 獲仔南填充率所需之任意大小者。 本發明之氧化鎂粒子之粒 祖于形狀並無特別限定，可列 舉針狀、棒狀、板狀、玻壯笠 ^ s . 狀專’較佳為更接近球狀之形狀。 τ〇Λ 藉由掃描型電子顯微鏡（JEOL 製 JSM840F)來觀察。 广豸氧化鎮粒子對粒徑並無特別限定，但平均-次粒 徑較佳為〇 . 1〜1 5 " m -r- 下限更佳為1 M m。即，如上所述 泛之粒徑範圍内之氧化鎂粒子可用作散熱材，且 “獲侍向填充率所需之任意大小者。 上述一次粒徑可藉 由以下實施例中詳細描述之方法來 測定。 2U1U1282 本發明之氧化鎂粒子較佳 粒子具有於與水接觸之情形時：面處理者。氧化錢 時易轉變為氫氧化鎂之性質。因此；濕潤環境下之情形 佳為實施表面處理。 此，為了提高耐水性，較 上述表面處理較佳為在 率低之狀態若疏水性的同時，維持導電 導電性者，則無法萨 所形成之被膜具有高 是用於電氣、電子^料之用化鎂之低導電率，因此特別 處理。f子材抖之用途時’較佳為進行特定之表面 根據上述觀點，上 所示之烷氧矽烷而進行 述表面處理較佳為藉 由下述通式（1)- The formation of human particles - U 丄 " 仏 之 人 人 人 人 人 人 人 人 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种 此种In the case where the median diameter/SSA diameter is 3 or less, more preferably 2.8 or less, and even more preferably 27 or less. Further, the magnesium oxide particles of the present invention are characterized in that since D90/D10 is 4 or less, the particle diameter thereof is The distribution is steep. If the particle size distribution is steep, it is easy to control the filling rate. Therefore, it is preferable to easily obtain a composition having high heat dissipation. The above 〇9〇/〇1〇 is more preferably 39 or less. The lean magnesium oxide particles of the present invention are characterized in that the number of primary particles is less than that of the prior oxidation-locking particles to form secondary particles, and D90 is compared with j (i.e., the particles are steeply distributed therefrom) Such magnesium oxide particles are not known, and are produced by the inventors of the present invention for the first time. The above-mentioned central control is also referred to as D5〇' means that the powder is divided into larger and smaller ones according to a certain particle size. The diameter of the measurement. The particle size is measured in the same manner as D ^ In the case of cloth, the particle size of the smaller one (4) 1〇% is called 201111282 DW, and the smaller one is 90%. The diameter of dm, ^ is obtained by measuring the particle size distribution. In the towel of the present invention, :: distribution is determined by the value of the laser diffraction particle size distribution measurement system Mic gift ac M Ding 33〇〇Εχ). The value obtained by the following premise: the particle is a sphere according to the specific surface area measured by the method of the inclusive method. The above magnesium oxide particles have no special heat limit for the particle size, but the diameter is preferably 〇 · 1 to 25 # m, the lower limit is more preferably 1 V m, that is, the magnesium oxide particles J in a wide range of particle diameters as described above are used as a heat dissipating material, and can be made into any of the high filling rates required by Jiang De. The size of the person. The above-mentioned magnesium oxide particles have no special heat limit for the particle size, but the SSA diameter is better than the U.1~15#m, and the lower limit is better for the horse 1", ie, as described above. In the wide range of particle sizes, the invitation #赶& ^ η η oxidized town puller can be used as a heat sink material, and can be made to obtain the south filling rate. Meaning the size of the person. The shape of the granules of the magnesium oxide particles of the present invention is not particularly limited, and may be a needle shape, a rod shape, a plate shape, or a glassy shape. The shape is preferably closer to a spherical shape. 〇Λ 观察 was observed by a scanning electron microscope (JSM 840 JJOL). The particle size of the granules is not particularly limited, but the average-secondary particle diameter is preferably 〇. 1 to 1 5 " m -r- The lower limit is more preferably 1 M m. That is, the magnesium oxide particles within the range of the particle size as described above can be used as the heat dissipating material, and "the size required for the filling rate can be obtained. The above primary particle diameter can be as described in detail in the following examples. 2U1U1282 The preferred particles of the magnesium oxide particles of the present invention have the property of being in contact with water: the surface treatment is easy to be converted into the property of magnesium hydroxide when oxidizing money; therefore, the surface treatment is preferably carried out in a wet environment. Therefore, in order to improve the water resistance, it is preferable that the surface treatment is such that if the conductivity is low and the conductive conductivity is maintained, the film formed by the Sa is not used for electrical and electronic materials. The low conductivity of magnesium is used, so it is specially treated. When it is used for the purpose of shaking, it is preferable to carry out the surface treatment according to the above-mentioned viewpoint, the alkoxysilane shown above is preferably treated by the following General formula (1)
Rl4-nSi(〇R2)n —(式中，表示碳數ι〜10之烧基、笨基或至少一部分 虱原子取代為氟之氟化烧基。示碳數卜3之院基1 表不2、3或4) 作為上述通式⑴所示之烧氧石夕院並無特別限定，例如 可列舉甲基二甲氧基矽烷、二甲基二甲氧基矽烷、苯基三 甲氧基矽烷、二苯二甲氧基矽烷、四乙氧基矽烷、甲基三 氧基夕烧一甲基一乙氧基石夕烧、苯基三乙氧基石夕燒、 正丙基三曱氧基矽烷、正丙基三乙氧基矽烷、己基三甲氧 基矽烷、己基三乙氧基矽烷、癸基三甲氧基矽烷、三氟丙 基三甲氧基矽烷等。 上述表面處理較佳為於表面形成相對於氧化鎮粒子為 0.1〜20質量％之被覆層。藉由進行此種處理，可在維持低 201111282 導電率之狀態下提高耐水性、耐酸性等。 如上所述之本發明之氧化鎂粒子可藉由於蝴酸或其鹽 存在下；^x燒虱氧化鎮而製造。此種氧化鎮粒子之製造方法 亦為本發明之一部分。藉由在此種蝴酸或其鹽存在下锻燒 所進行之氧化鎂之製造於以下方面較佳：藉由調整硼酸或 其鹽之添加量及煅燒溫度，可容易地獲得具有上述特定（中 徑）/ (SSA徑）之比及D90/ D ! 〇、且具有所需粒徑之氧化鎂。 更具體而言，可藉由以下詳細描述之本發明之氧化鎂 粒子之製造方法而獲得。 μ卜，砰細描述上述本發 本發明之氧化鎂粒子之製造方法中，使用氣氧化鎮作 為原料。上述氫氧化鎂較佳為平均粒徑〇 〇5〜2 V爪。上述 〃氧化鎂之平均粒徑係藉由雷射繞射粒度分佈測定裝置(日L 機裝股份有限公司製Ml⑽trac MT测Εχ)所測定之值。 本叙明中使用之氫氧化鎂係粉碎天然礦物而獲得之天 =品、或藉由於水中以驗性物質中和水溶性鎮 =品等:其由來並無任何限定，但較佳為使用後者之合 -於製造合成品之情形時’作為上述 ❹例如氯化鎮、硫酸鎮、㈣、乙酸鎖等…作： =生物質’可使用例如氯氧化納、氨氧化鉀、氨等。 於〇8〜Γ鹼性物質通常相對於水溶性❹1當量， ；.1.2當量之範圍内使用。 本發明争，於在水中使水 —情形時，為使水= 201111282 2 Vm、比表面積為1 |·生物質〇. 8〜1.2當量反應，較佳為與驗性物冑l 〇〜1 2當 量反應’獲得含有氫氧化減澱之輯，進行在加壓下溫 200 C之範圍内加熱該漿料之水熱處理繼而將 所得之反應混合物通常冷卻至f溫’進行過據'水洗而去 除副生鹽’進行乾燥、粉碎，通常獲得平均—次粒徑為 g之範圍的具有六角板狀 30 之形狀的氫氧化鎂，藉由锻燒該等，通常可獲得平均一次 粒徑為0.1〜2 之範圍的球狀氧化鎖粒子。 本發明之氧化鎮粒子之製造方法之特徵在於：於删酸 或其鹽之存在下進行炮燒。無機粒子之製造中，為了辦大 粒徑，而有在助炫劑存在下進行般燒之情況。本發明㈣ 人發現，若使用石朋酸或其鹽作為此種锻燒時之助炼劑，則 與使用其他化合物作為助炼劑之情形時相比，所獲得之氧 化鎂粒子之粒徑分佈陡峭。 上述蝴酸或其鹽較佳為設為相對於氣氧化鎮⑽ 份以删換算為〇丨〜⑺莫 、卞 关斗份右未滿0.1莫耳份，則粒子 難以成長’故能量消耗變高。若超過10莫耳份，則粗粒子 :產生變多，產品之良率下降，生產性不I藉 述蝴酸或其鹽之摻合量及反應溫 ^ , ^ J獲仵具有所需粒徑 之軋化鎂粒子。於欲縮小粒徑之情 4甘 了牧佳為減少硼酸 或其皿置，降低反應溫度，於欲增大粒徑之情形時，較佳 為增多硼酸或其鹽量，提高反應溫度。 作為上述石朋酸或其鹽並無特別限定’例如可列 酸、硼酸鋅—3.5水合物、硼酸銨—八k人 软八水合物、硼酸鉀、硼 10 201111282 西欠鈣一 η水合物 '硼酸三乙醇胺、硼酸鈉、硼酸鎂—〇水合 蝴酸鐘四爛酸知：—四水合物、四棚酸鈉、四蝴酸納 —十水合物、四硼酸鉀—四水合物、四硼酸錳（11)、無水四 硼酸鋰、四爛酸經—η水合物等。作為上述剛^鹽，既可為 水合物，亦可為無水物。作為上述硼酸或其鹽，較佳為四 朋歐鋰五水合物、四硼酸鈉—_h水合物、四硼酸鉀〜四 水合物及四硼酸銨—四水合物，其中較佳為四硼酸鈉—十 水合物（硼砂）。 丁 於使用W酸鹽4乍為上述硼酸或其鹽《情形日夺，亦可 對於氫氧化鎂混合硼酸與金屬鹽化合物及，或金屬氫 物。又，亦可使用硼酸與録鹽及/或氨水溶液。即 IS: - 化鈉、鐘鹽、氫氧化鐘、鉀鹽、氫氧化鉀、 :I ’合液、鋅鹽、三乙醇胺鹽等胺鹽化合物等略類 及/或金屬氫氧化物與 '^頬 蒋r太路β… 虱氧化鎂中，同樣亦可 獲付本發明之氣化鎂。於此種 鹽類及/布仝崎將蝴酸與 1類及金屬^^化物添 在不同階段分別添加（例如化合’亦可 等）。 在煅燒之中途添加其中—者 :發明之氧化鎮粒子可藉由 酸或其鹽以公知之方 < 虱孔化鎂與上述硼 造。作為上述混合並二炮燒所得之混合物而製 式混合。上述煅燒於工# 疋車乂佳為使用分散劑之濕 限定。 、〃上較佳為靜置炮燒，但並無特別 上述锻燒係於_〜咖t 右於未滿1 0 〇 〇 °c時 201111282 炮燒，則於粒子成再 于或長不充分方面不佳。若超過18〇〇<t，則 粗大粒子之產生變多， 夕於有收率下降之虞方面不佳。上述 溫度亦係對所得氡化 化鎮粒子之粒徑產生較大影響的要素， 因此較佳為根據目；2 , h之拉子之粒徑於上述溫度範圍内選擇 適當之溫度。 s i述方法所製造之氡化鎂粒子，雖其粒徑分佈陡 肖’但於需要獲得更陡哺 者之情形時，或為了去除以低比 例所含有之粗大粒子 ^ Λ 子亦可利用粉碎、薛選來進行分級。 私碎方法並無特別限定 例如可列舉霧化器等。又作為利 用4選所進行之分級方法，可 舉濕式分級、乾式分級。 發明之氧化鎮粒子對於盆田、全斗卜 γm τ π其用途並無特別限定，例如 可適用於散熱性填料之用全 之一部八。 途。此種散熱性填料亦為本發明 本發明之散熱性填料诵杳 勒執H心 使用於散熱性樹脂組成物或 散熱性潤滑脂、散熱性塗 ^ 公知女齡，…Η 科4。關於此種用途，存在多個 Α去文獻，本發明之散熱性 樹脂組成物或散埶性潤,、M ;纟種公知的散熱性 、、r生潤'月月旨 '散熱性塗料。 使用本發明之氧化鎂粒 均滿足本發明之必要條件，/為散熱性填料之情形時， 鎮粒子昆合使用。更Me可將粒徑不同之複數個氧化 之氧化鎖粒子：以其粒徑比為了方式所侍 藉由使用以上述電子顯微铲昭々⑽0之比例選擇 測定方法而求得之_次粒徑置所彳自攝之圖像之 0.05〜4 之氧化鎂（b)，二〜15 之氧化鎂⑷與 乂（a) . (b)為 5 : 5 〜9 : 1 之重 12 201111282 量比率進行混合。 又，亦可組合3種以上之氧化鎂粒子。於組合 化鎮粒子之情形時，係組合使用藉由使用以上 = 鏡照片拍攝裝置所拍攝之圖像之測定 頦微 徑為1〜15 之氧㈣⑷、G()5 之:之—次粒 叫V m之氧化鎂（b)、 〇·01〜1 P之氧化鎮⑷，可舉出藉由如下方式所得之氧 化鎮粒子：選擇其粒徑比為^⑷/(b)㈣、^(bRl4-nSi(〇R2)n - (wherein, a fluorinated group of a carbon group of 1-4 to 10, a stupid group or at least a part of a ruthenium atom substituted with fluorine is used. 2, 3 or 4) The oxygen-burning stone shown in the above formula (1) is not particularly limited, and examples thereof include methyl dimethoxy decane, dimethyl dimethoxy decane, and phenyl trimethoxy decane. , diphenyl dimethoxy decane, tetraethoxy decane, methyl trioxy oxime, monomethyl ethoxy cerium, phenyl triethoxy cerium, n-propyl tridecyl decane, N-propyltriethoxydecane, hexyltrimethoxydecane, hexyltriethoxydecane, decyltrimethoxydecane, trifluoropropyltrimethoxydecane, and the like. The surface treatment is preferably a coating layer having a surface of 0.1 to 20% by mass based on the oxidized town particles. By performing such a treatment, it is possible to improve water resistance, acid resistance, and the like while maintaining a low conductivity of 201111282. The magnesium oxide particles of the present invention as described above can be produced by the presence of a caustic acid or a salt thereof; The method of producing such oxidized town particles is also part of the invention. The production of magnesium oxide by calcination in the presence of such a cyanic acid or a salt thereof is preferably as follows: by adjusting the addition amount of boric acid or a salt thereof and the calcination temperature, the above specific (middle) can be easily obtained. Magnesium oxide having a desired particle size and a ratio of D//S! More specifically, it can be obtained by the method for producing magnesium oxide particles of the present invention described in detail below. In the method for producing the magnesium oxide particles of the present invention, the gas oxidation town is used as a raw material. The above magnesium hydroxide is preferably an average particle diameter of 〜 5 to 2 V claws. The average particle diameter of the above-mentioned magnesium oxyhydroxide is a value measured by a laser diffraction particle size distribution measuring apparatus (Ml (10) trac MT manufactured by N. L. Machine Co., Ltd.). The magnesium hydroxide used in the present invention is a product obtained by pulverizing a natural mineral, or a water-soluble town product by an inert substance in water, and the like: the origin thereof is not limited, but the latter is preferably used. In the case of manufacturing a synthetic product, 'as the above-mentioned hydrazine, for example, chlorinated town, sulphuric acid town, (iv), acetic acid lock, etc.: = biomass can be used, for example, sodium oxychloride, potassium oxyhydroxide, ammonia, and the like. The 〇8~Γ alkaline substance is usually used in the range of 1 equivalent of water-soluble hydrazine; 1.2 equivalent. The present invention contends that in the case of water in the water - in the case of water = 201111282 2 Vm, specific surface area is 1 | · biomass 〇 8~1.2 equivalent reaction, preferably with the test substance 胄 l 〇 ~ 1 2 The equivalent reaction 'obtains a series containing hydroxide precipitation, performs hydrothermal treatment of heating the slurry in a temperature range of 200 C under pressure, and then the resulting reaction mixture is usually cooled to f temperature'. The raw salt 'dried and pulverized, and usually has a shape of a hexagonal plate shape 30 having an average-secondary particle size in the range of g. By calcining, etc., an average primary particle diameter of 0.1 to 2 is usually obtained. A range of spherical oxidative lock particles. The method for producing oxidized particles according to the present invention is characterized in that the calcination is carried out in the presence of acid or a salt thereof. In the production of inorganic particles, in order to achieve a large particle size, it is usually burned in the presence of a builder. According to the invention (4), it has been found that when staphic acid or a salt thereof is used as the fluxing agent in the calcination, the particle size distribution of the obtained magnesium oxide particles is compared with the case of using other compounds as a refining agent. Steep. It is preferable that the above-mentioned cyanic acid or a salt thereof is converted to 〇丨~(7) Mo, and 卞 Guandoufen is less than 0.1 mol% with respect to the gas oxidation town (10), and the particles are hard to grow, so the energy consumption is high. If it exceeds 10 moles, the coarse particles will be more and more, the yield of the product will decrease, and the productivity will not be described by the amount of the acid or its salt and the reaction temperature. Rolled magnesium particles. In order to reduce the particle size, it is preferable to increase the amount of boric acid or its salt and increase the reaction temperature in order to reduce the reaction temperature in order to reduce the boric acid or its dish. The above-mentioned sphagic acid or a salt thereof is not particularly limited, for example, 'colic acid, zinc borate-3.5 hydrate, ammonium borate-eight k-person soft octahydrate, potassium borate, boron 10 201111282 sulphur-n-hydrate hydrate' Boric acid triethanolamine, sodium borate, magnesium borate - hydrazine hydrated acid clock, four rotten acid known: - tetrahydrate, sodium sulphate, tetrasodium sulphate - decahydrate, potassium tetraborate - tetrahydrate, manganese tetraborate (11), anhydrous tetraborate, tetrazolium acid, η hydrate, and the like. The above salt may be either a hydrate or an anhydride. The boric acid or a salt thereof is preferably tetrapone lithium pentahydrate, sodium tetraborate-_h hydrate, potassium tetraborate to tetrahydrate, and ammonium tetraborate-tetrahydrate, of which sodium tetraborate is preferred. Decahydrate (borax). The use of W salt 4 is the above-mentioned boric acid or a salt thereof. It is also possible to mix boric acid with a metal salt compound and metal hydrogen for magnesium hydroxide. Further, boric acid and a salt of a salt and/or an aqueous ammonia solution can also be used. That is, IS: - sodium, bell, hydrazine, potassium, potassium hydroxide, : I 'liquid, zinc salt, triethanolamine salt and other amine salt compounds and/or metal hydroxides and '^ In the case of magnesium oxide, the magnesium oxide of the present invention can also be obtained. In such a salt and/or cloth, the acid is added to the class 1 and the metal compound at different stages (for example, compounding or the like). It is added in the middle of calcination: the oxidized town particles of the invention can be produced by using an acid or a salt thereof in a well-known manner of <porous magnesium. The mixture was mixed as a mixture of the above-mentioned mixed and second-fired. The calcination described above is defined by the wetness of the dispersant. It is better to stand still and burn, but there is no special calcination in the _~ coffee t right to less than 1 0 〇〇 °c 201111282 cannon burning, in terms of particle formation or length is not sufficient Not good. If it exceeds 18 〇〇 < t, the generation of coarse particles becomes large, and it is not good in terms of a decrease in yield. The above temperature is also an element which greatly affects the particle size of the obtained deuterated town particles. Therefore, it is preferred to select the appropriate temperature within the above temperature range according to the particle size of the 2, h. The magnesium telluride particles produced by the method described above have a sharp particle size distribution, but they may be pulverized when it is necessary to obtain a steeper donor or to remove coarse particles contained in a low ratio. Xue Xuan came to grade. The method of smashing is not particularly limited. For example, a nebulizer or the like can be cited. Further, as a classification method using the four-choice, it is possible to carry out wet classification and dry classification. The oxidized town particles of the invention are not particularly limited in their use for pots and hoppers γm τ π , and for example, they can be applied to all of the heat-dissipating fillers. way. The heat-dissipating filler of the present invention is also a heat-dissipating filler of the present invention, which is used for a heat-dissipating resin composition or a heat-dissipating grease, and a heat-dissipating coating. Regarding such use, there are a number of derogatory documents, a heat-dissipating resin composition of the present invention, or a dampening property, M, a known heat-dissipating property, and a heat-dissipating paint. The use of the magnesium oxide particles of the present invention satisfies the requirements of the present invention, and in the case of a heat-dissipating filler, the town particles are used in combination. Further, Me can oxidize a plurality of oxidized oxidized particles having different particle diameters: the particle size ratio is obtained by using the above-mentioned electron microsurgical shovel (10) 0 ratio measurement method to obtain the _ secondary particle diameter Magnesium oxide (b) of 0.05 to 4, 2 to 15 mg of magnesium oxide (4) and yttrium (a). (b) 5:5 to 9: 1 weight 12 201111282 mixing. Further, three or more kinds of magnesium oxide particles may be combined. In the case of combining the town particles, the combination of the images taken by using the above-mentioned mirror photo taking device is used to measure the oxygen having a micro-path of 1 to 15 (4), (4), G()5: The oxidized town (4) of magnesium oxide (b) and 〇·01~1 P of V m may be oxidized particles obtained by the following method: the particle size ratio is selected to be ^(4)/(b)(d), ^(b)
$20之比例之粒子，相對於氧化鎂總量，以⑷：⑽C =5:5〜9:1、(b):(C)=5:5〜Μ之重量比率進行遇合。 如上所述，藉由選擇填充率變高之組合而混合粒徑不 冋之複數個氧化鎖粒子，可獲得高填充率，於可 之散熱性能方面較佳。 獲侍優異 將本發明之氧㈣粒子料散熱性填料之情形時，亦 氧Li其他成分。作為可併用之其他成分，可列舉氧化鋅、 ，鈦、氧化料金屬氧化物，氮㈣、氮化硼、碳化石夕、 二二Η:化鈦 '金屬石夕、金剛石等氧化鎂以外之散熱性 真科树月曰、界面活性劑等。 將上述氧域粒子用作散熱性填料之 與樹脂混合而成之槲浐έ日士、仏+ 丁 J作雨 為太鉻0成之樹月曰組成物而使用。此種樹脂組成物亦 朽^之一。於此情形時，所使用之樹脂既可為熱塑性 :二1可為熱硬化性樹脂，可列舉絲樹脂、盼類樹脂、 :L ·' (PPS)樹脂、聚酯系樹脂、聚醯胺、聚醯亞胺、聚 Γ樹r、平聚乙烯、聚丙烯、聚氣乙烯、聚偏二氯乙烯、碳 日"基丙烯酸”旨、乙烯一丙烯酸乙醋共聚物(eea) 13 201111282 樹脂、聚碳酸酯、聚胺基曱酸酯 '聚縮醛、聚苯謎、聚趟 醯亞胺、丙烯腈一丁二烯一苯乙烯共聚物（ABS)樹脂、液晶 樹脂（LCP)、矽樹脂、丙烯酸樹脂等樹脂。 本發明之樹脂組成物可為以下之任一形態：藉由在溶 融狀態下混練熱塑性樹脂與上述氧化鎂粒子所獲得之熱成 型用樹脂組成物；混練熱硬化性樹脂與上述氧化鎂粒子 後，藉由加熱硬化而獲得之樹脂組成物等。 本發明之樹脂組成物中之上述氧化鎂粒子之摻合量， 可根據目標導熱率或樹脂組成物之硬度等樹脂組成物的性 能而任意地決定。為了充分地發揮上述氧化鎂粒子之散熱 性能，較佳為相對於樹脂組成物中之固形物成分總量含有 10〜9.0體積％。上述摻合量可視必要之散熱性能進行調整 來使用’於要求更冋散熱性之用途中較佳為含有3 G體積％ 以上’更佳為50體積％以上。 本發明之樹脂組成物可根據用途自由地選擇樹脂成 刀。例如’在安裝於熱源與散熱板之間並使其密接之情形 時’選擇石夕樹脂或丙豨酸樹脂之類的黏著性高、硬度低之 伞赞明之樹 .....，〜工/3曰組风初之 時’例如可藉由如下等方法而製造熱塑性樹脂與上述 鎮粒子由使用螺旋型雙轴擠出機之炫融混練，使 =物顆粒化，其後藉由射出成型等任意之成形方法 形為所需形狀。 本發明之樹脂組成物係將熱硬化性樹脂與上述氧 14 201111282 :子混練後、藉由加熱硬化而獲得之樹脂組成物之情形 日’ ’例如較佳為藉由加壓成形等而成形者。此種樹脂 物之製造方法並無特別限定’例如可藉由 組成物成型而製造。 〜忧树月曰 本發明之樹脂組成物之用途有電子零件之散熱構件、 :填充劑、用於溫度測定等之絕緣性填充劑等。例如， 發明之樹脂組成物可用以將來自Mpu、功率電晶體 壓器等發熱性電子零件的献傳 勒“ 散熱片或散熱風扇等散 :轉，可於發熱性電子零件與散熱零件之間夹持使用。 ^ 此成發熱性電子零件與散熱零件間之傳熱變得良好，可 / =發熱性電子零件之誤動作。可適用於熱管與散熱 盗之、《組入有各種發熱體之模組與散熱器之連接。 ，用上述氧化鎖粒子作為散熱性填料之情形時，亦可 :為與3有礦物油或合成油之基礎油混合而成之散 μ脂來使用。此種散熱性潤滑脂亦為本發明之一。 本發明之散熱性潤滑脂中之上述鎮粒子之換合量可根 據目標導熱率而任意地決定。 ' 鎂粒子之散熱性能，較佳為相對也表現出上述氧化 10〜90體積％以上。上述搀合量 3有 ，敕A麻田认 視必要之散熱性能進行 ㈣來❹，於要求更高散純之_巾，較 體積％以上，更佳為50體積0/〇以上。 '、有 成、由上m可組合使用1種或2種以上之礦物油、合 佳作=炫油等各種油性材料。作為合成油，特 佳為L油。作為合成油，可使 使用α —烯烴、二醋、多元醇 15 201111282 酯、偏苯三酸酯、聚苯蜮、烷基苯基醚等。 本發明之散熱性潤滑炉 ^ Α μ ·+· R 亦了視需要含有界面活性劑。 …述界面活性劑，較佳為非離子系界面活性劑。藉由 非離子系界面活性劑之摻合， 當地控制稍度。 了謀“導熱率化，且可適 作^非離子系界面活性劑，可列舉聚氧乙稀烧基輕、 mi本基謎、聚氧乙稀烧基蔡基鱗、聚氧乙稀化 蓖麻油、聚氧乙烯氫化鍵府 以油、聚氧乙料基醯胺'聚氧 乙稀-聚氧丙稀二醇、聚氧乙稀—聚氧丙稀二醇乙二胺、 十甘油脂肪酸酿、聚氧乙烯單脂肪酸醋、聚氧乙浠二脂肪 “、聚氧乙稀丙二醇脂肪酸龜 '聚氧乙稀山 脂肪酸醋、聚氧乙稀山梨糖醇針三脂肪酸醋、乙二醇單脂 肪酸醋、〔乙二醇單脂肪酸醋、丙二醇單脂肪酸自旨、甘油 單脂肪酸酿、季戍四醇單脂肪酸醋、山梨糖醇肝單脂肪酸 酿、山梨糖醇奸倍半脂肪酸醋、山梨糖醇肝三脂肪酸醋。 非離子系界面活性劑之添加效果係根據表示散熱性填 料之種類、摻合量、及親水性與親油性之平衡之HLB(親水 親油平衡）而不同。於本實施形態中所使用之非離子系界面 活性劑中’為了於室溫下亦獲得良好之稠度，較佳為hlb 為9以下之液狀界面活性劑。又，於不重視高散熱性潤滑 脂等之電絕緣性或電阻下&之用途中，引吏用陰離子系界 面活性劑、陽離子系界面活性劑、兩性界面活性劑。、 本發明之散熱性潤滑脂可藉由使用調麵機（捏合機”框 式混合器'行星式攪拌機等混合機器混合上述成分而製備。 16 201111282 本發明之散熱性潤滑脂係藉由塗佈於發熱體或散熱體 上而使用。作為發熱體，例如可列舉一般之電源；電源用 力率電曰曰體、功率模組、熱阻器、熱電偶、溫度感測器等 電子設備；LSI、CPU等積體電路元件等發熱性電子零件等。 f為散熱體，例如可列舉散熱片、散熱器等散熱零件；熱 s散熱板等。塗佈可藉由例如網版印刷進行。網版印刷 可使用例如金屬掩模或筛目進行。藉由將本發明之散熱性 潤滑脂***並塗佈於發熱體及散熱體之間，可自上述發埶 體向上述散熱體有效地導熱，因此可有效地去除來自上述 發熱體之熱。 ,於使用上述氧化鎮粒子作為散熱性填料之情形時，可 製成分散於樹脂溶液或分散液中之塗料組成物而使用。此 種散熱性塗料組成物亦為本發明之一。於此種情形時，所 使用之樹脂既可具有硬化性，亦可不具有硬化性。作為上 述樹脂，具體而言可列舉作為可使用於上述樹脂組成物中The particles of the ratio of $20 are taken up in a weight ratio of (4): (10) C = 5: 5 to 9:1, (b): (C) = 5:5 to Μ with respect to the total amount of magnesium oxide. As described above, by selecting a combination of a high filling ratio and mixing a plurality of oxidized lock particles having a small particle diameter, a high filling ratio can be obtained, which is preferable in terms of heat dissipation performance. Excellent in the case of the oxygen (tetra) particle material heat-dissipating filler of the present invention, other components of oxygen Li. Examples of other components that can be used together include heat dissipation other than zinc oxide, titanium, an oxide metal oxide, nitrogen (tetra), boron nitride, carbon carbide, or bismuth: titanium oxide, metal oxide, and diamond. Sexual science tree scorpion, surfactant, etc. The above-mentioned oxygen domain particles are used as a heat-dissipating filler and are mixed with a resin, and they are used as a composition of a chrome-based sap. This resin composition is also one of the defects. In this case, the resin to be used may be thermoplastic: two may be a thermosetting resin, and examples thereof include silk resin, expectant resin, :L · ' (PPS) resin, polyester resin, polyamine, Polyimide, polyeucalyptus r, flat polyethylene, polypropylene, polyethylene, polyvinylidene chloride, carbon day "acrylic acid, ethylene acrylate copolymer (eea) 13 201111282 resin, Polycarbonate, polyamino phthalate 'polyacetal, polyphenylene, polyimide, acrylonitrile butadiene styrene (ABS) resin, liquid crystal resin (LCP), enamel resin, A resin composition such as an acrylic resin. The resin composition of the present invention may be any one of the following: a resin composition for thermoforming obtained by kneading a thermoplastic resin and the magnesium oxide particles in a molten state; and kneading a thermosetting resin and the above The resin composition obtained by heat curing after the magnesium oxide particles, etc. The amount of the magnesium oxide particles blended in the resin composition of the present invention may be a resin composition such as a target thermal conductivity or a hardness of the resin composition. Performance and arbitrarily In order to sufficiently exhibit the heat dissipation performance of the above magnesium oxide particles, it is preferably contained in an amount of 10 to 9.0% by volume based on the total amount of the solid content in the resin composition. The above-mentioned blending amount may be adjusted by using necessary heat dissipation properties to be used. In the application requiring more heat dissipation, it is preferably contained in an amount of 3% by volume or more and more preferably 50% by volume or more. The resin composition of the present invention can be freely selected from a resin according to the use, for example, 'installed in a heat source and When the heat sinks are in close contact with each other, 'Select a tree with high adhesion and low hardness, such as Shi Xi resin or acrylic acid resin.....,~工/3曰组风初之之For example, the thermoplastic resin can be produced by the following method, and the above-mentioned town particles can be pulverized by the use of a spiral type twin-screw extruder to granulate the granules, and then formed into an arbitrary molding method by injection molding or the like. The resin composition of the present invention is a case where the resin composition obtained by kneading the thermosetting resin and the above-mentioned oxygen 14 201111282 is cured by heat curing, for example, preferably by adding The method of producing the resin is not particularly limited. For example, it can be produced by molding a composition. ~ 忧树月曰 The use of the resin composition of the present invention includes a heat dissipating member for an electronic component, : filling An insulating filler for use in temperature measurement, etc. For example, the resin composition of the invention can be used to disperse heat-generating electronic components such as Mpu and power transistor presses from "heat sinks or cooling fans: Turn, can be used between the heat-generating electronic parts and the heat-dissipating parts. ^ The heat transfer between the heat-generating electronic parts and the heat-dissipating parts becomes good, and the malfunction of the heat-generating electronic parts can be made. It can be applied to heat pipe and heat dissipation. It is a combination of modules and radiators with various heating elements. In the case where the above oxidized lock particles are used as the heat-dissipating filler, it may be used as a mixture of three kinds of base oils which are mixed with a base oil of mineral oil or synthetic oil. Such a heat-dissipating grease is also one of the inventions. The blending amount of the above-mentioned town particles in the heat-dissipating grease of the present invention can be arbitrarily determined depending on the target thermal conductivity. The heat dissipation performance of the magnesium particles is preferably such that the above oxidation is also 10 to 90% by volume or more. The above-mentioned blending amount is 3, and 敕A Ma Tian recognizes the necessary heat-dissipating performance. (4) It is required to be higher in volume and more than 50% by volume. ', and it is possible to use one or two or more kinds of mineral oils from the top m, and it is a combination of various oily materials such as a good oil. As the synthetic oil, L oil is particularly preferred. As the synthetic oil, an α-olefin, a diacetate, a polyol 15 201111282 ester, a trimellitic acid ester, a polyphenyl hydrazine, an alkylphenyl ether or the like can be used. The heat-dissipating lubricating furnace of the present invention ^ Α μ ··· R also contains a surfactant as needed. The surfactant is preferably a nonionic surfactant. The local control is slightly controlled by the blending of nonionic surfactants. It is intended to be "thermal conductivity" and can be used as a non-ionic surfactant. Examples include polyoxyethylene dilute base, mi-based mystery, polyoxyethylene dilute base, and polyoxyethylene castor oil. Polyoxyethylene hydrogenation bond oil, polyoxyethylene decylamine 'polyoxyethylene-polyoxypropylene glycol, polyoxyethylene-polyoxypropylene glycol ethylenediamine, decaglycerin fatty acid, Polyoxyethylene mono-fatty acid vinegar, polyoxyethylene hydrazine di-fat", polyoxyethylene propylene glycol fatty acid turtle 'polyoxyethylene rare mountain fatty acid vinegar, polyoxyethylene sorbitol needle three fatty acid vinegar, ethylene glycol mono-fatty acid vinegar, [Ethylene glycol mono-fatty acid vinegar, propylene glycol mono-fatty acid self-purpose, glycerin mono-fat brewing, quaternary tetraol mono-fatty vinegar, sorbitol liver mono-fat brewing, sorbitol sesquitercene fatty acid vinegar, sorbitol liver tri-fatty acid vinegar. The addition effect of the nonionic surfactant differs depending on the type of the heat-dissipating filler, the blending amount, and the HLB (hydrophilic-lipophilic balance) which is a balance between hydrophilicity and lipophilicity. In the nonionic surfactant used in the present embodiment, in order to obtain a good consistency at room temperature, a liquid surfactant having a hlb of 9 or less is preferable. Further, an anionic surfactant, a cationic surfactant, and an amphoteric surfactant are used for the electrical insulating properties of the high heat-dissipating grease or the like. The heat-dissipating grease of the present invention can be prepared by mixing the above components using a mixing machine such as a dough mixer (kneader) frame mixer, planetary mixer, etc. 16 201111282 The heat-dissipating grease of the present invention is coated by the coating. It is used for a heating element or a heat sink. Examples of the heating element include a general power source, an electric power source, an electric power unit, a power module, a thermal resistor, a thermocouple, and a temperature sensor; A heat generating electronic component such as an integrated circuit component such as a CPU, etc. f is a heat radiating body, and examples thereof include a heat dissipating member such as a heat sink and a heat sink, a heat s heat dissipating plate, etc. The coating can be performed by, for example, screen printing. It can be carried out, for example, by using a metal mask or a mesh. By inserting and applying the heat-dissipating grease of the present invention between the heat generating body and the heat radiating body, heat can be efficiently conducted from the hairpin body to the heat sink body, thereby The heat from the heat generating body is effectively removed. When the oxidized town particles are used as the heat-dissipating filler, the coating composition dispersed in the resin solution or the dispersion can be used. The heat-dissipating paint composition is also one of the inventions. In this case, the resin to be used may or may not have curability. The resin may be specifically used as the resin. In the above resin composition
之樹脂所例示之樹脂。塗料gf I & A T曰孟行既可為含有有機溶劑之溶劑系 者，亦可為於水中樹脂溶解或分散之水系者。 上述塗料組成物之製造方法並無特別限定，例如可藉 由使用分散機或珠磨機等將必要之原料及溶劑混合、分散 而製造。 本發明之散熱性塗料組成物中之上述氧化鎂粒子的摻 合量可根據目標導熱率而任意地決定。為了充分地表現出 上述氧化鎂粒子之散熱性能，較佳為相對於塗料組成物總 量含有^9〇體積％以上。上述摻合量可視必要之散熱性 17 201111282 能進行調整來使用，於要求更高之斟舶ω >又同 < 散熱性之用途中，較佳 為含有30體積％以上，更佳為5〇體積％以上。 本發明t氧化鎮粒子，除上述散熱性填料之以外，亦 可用於橡膠之硫化促進劑；塗料、油墨用顏料；冑藥品尊 領域。 [實施例] 以下列舉實施例來說明本發明 令赞明，但本發明並不受該黧 實施例任何限定。 以下，獲得之氧化鎂粒子之中徑及粒度分佈係以雷射 ，·堯射粒度分佈測定裳置（日機裝股份有限公司製Microtrac MT 3300 EX)來測定。 (氧化鎂之一次粒徑之測定方法） 首先’由BET比表而接；^古，| ^ 面積及真比重求得粒徑（SSA粒徑）。 然後利用掃描型電子顯料The resin exemplified by the resin. The coating gf I & A T曰 Meng Xing can be either a solvent containing an organic solvent or a water system in which the resin is dissolved or dispersed in water. The method for producing the coating composition is not particularly limited. For example, it can be produced by mixing and dispersing a necessary raw material and a solvent using a disperser or a bead mill. The blending amount of the above-mentioned magnesium oxide particles in the heat-radiating coating composition of the present invention can be arbitrarily determined depending on the target thermal conductivity. In order to sufficiently exhibit the heat dissipation performance of the above-mentioned magnesium oxide particles, it is preferable to contain 9% by volume or more based on the total amount of the coating composition. The above-mentioned blending amount can be adjusted and used according to the necessary heat dissipation property 17 201111282, and it is preferably 30% by volume or more, and more preferably 5, in the use of the higher heat dissipation. 〇 5% by volume or more. The t-oxidized town particles of the present invention, in addition to the above-mentioned heat-dissipating filler, can also be used as a vulcanization accelerator for rubber; a pigment for coatings and inks; and a drug-respecting field. [Examples] The following examples are given to illustrate the present invention, but the present invention is not limited to the examples. In the following, the diameter and particle size distribution of the obtained magnesium oxide particles were measured by laser and particle size distribution measurement (Microtrac MT 3300 EX manufactured by Nikkiso Co., Ltd.). (Method for Measuring Primary Particle Size of Magnesium Oxide) First, the particle diameter (SSA particle diameter) was determined by the BET ratio table; Then using scanning electronic materials
Tc ”肩臧鏡照片拍攝裝置（JEOL·製 JSM840F) ’於SSA粒徑為1〇 "各 .. # m左右之情形時，以2000Tc "Shoulder mirror photo camera (JMOL·JSM840F)" when the SSA particle size is 1〇 " each .. # m or so, 2000
倍之倍率進行5視野拍攝，於Q n ?攝於SSA粒徑為1 及2 左右之情形時’以5000倍之俾盅 _The magnification is 5 fields of view, and when Q n is taken in the case where the SSA particle size is about 1 or 2, it is 5,000 times _ _
...^ 之七率進仃5視野拍攝，於SSA 拉！為〇·1 /z m左右之愔形眭 月开y時’以50000倍之倍率進行5 於 ，圖像部分為短邊9⑽、長邊12⑽之照片。對 邊、#自各條短邊及長邊之中間點分別才目對於短 邊 '長邊引出平行線，逸 R ^ 進而引出兩條對角線，使用游標卡 尺測定重疊於共計四條直 腌访 、^上之粒子之短徑及長徑之值， 4值之平均值作為其 ,也 国像之平均一次粒徑（SEM徑）。 (實施例1)氧化鎂粒子〜a 18 201111282 將堺化學工業製氫氧化鎂（產品名MGZ_ kg添加至 溶解有Dispex A40(Allied Colloid公司製聚丙烯酸銨鹽）5() g、四硼酸鈉一十水合物（和光純藥製μ.64 g之離子交換水及 L中，製成氫氧化鎂之分散漿料。此時添加之四硼酸鈉—十 水合物之量以硼換算為Ο·〗爪〇1份。將該漿料喷霧乾燥，而 獲得均勻地混合有四删酸鈉—十水合物之氮氧化鎮。將該 氫氧化鎂放入帶蓋之氧化鋁匣缽坯中，於11〇〇。〇進行小 時之大氣锻燒。對锻燒後之氧化錢行脫鹽處理後，進^ 粉碎而獲得氧化鎮粒子-a。由該氧化鎮粒子_3之照 片求得之-次粒徑為1.68 " m、由粒度分佈求得之中徑為 。…、由比表面積算出之比表面積徑為16…，由 粒度分佈求得之中徑/由矣品接七 /田比表面積求得之比表面積徑之值 為 2_60 〇 又 ’ D90 為 6.79 ν m，D10 Α ^ μ m 為 1·75 β m > D9〇/ DIO之值為3.88。 (實施例2)氧化鎂粒子—b 除了將明酸鈉—十水合物之量設為8.20 g以外，進 行與實施例1相同之操作’獲得氧化錤粒子4。此時添加 之四硼酸鈉--^水合物之量以械曾* Λ 里乂删換算為〇·5 mol份。由該氧 化鎮粒子一b之SEM昭>{电ί曰> ,, ‘，、、月衣传之一次粒徑為2.06 μ m、由 粒度分佈求得之中徑為3 91 , . Mm、由比表面積算出之比表 面積徑為1.98 yin，由粒ρ八&七+ +、 孤度刀佈求得之中徑/由比表面積 求得之比表面積徑之值為丨 y,又，D90 為 6.22 μ m , Dl〇 為 2.35 D9〇/Dl〇 之值為 2 65。...^ The rate of seven is taken in 5 field of view, pulled in SSA! It is a 愔·1 /z m 愔 眭 眭 眭 y y 眭 y y y 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 500 以 以 以 以 以 以 以 以 以 以 以 以 以For the side, # from the short side of each short side and the long side of the long side, respectively, for the short side 'long side to draw parallel lines, escape R ^ and then lead two diagonal lines, using vernier calipers to measure overlap with a total of four straight picking, The value of the short diameter and the long diameter of the upper particle, the average value of the four values is taken as the average primary particle diameter (SEM diameter) of the national image. (Example 1) Magnesium oxide particles ~ a 18 201111282 Magnesium hydroxide produced by 堺Chemical Industry Co., Ltd. (product name MGZ_ kg was added to dissolve Dispex A40 (ammonium polyacrylate of Allied Colloid) 5 () g, sodium tetraborate Decahydrate (a total of 64 g of ion-exchanged water and L made by Pure Chemicals) is used as a dispersion slurry of magnesium hydroxide. The amount of sodium tetraborate-decahydrate added at this time is converted into boron in terms of boron. 1 part of Xenopus. The slurry is spray-dried to obtain a nitrogen-oxidized town uniformly mixed with sodium tetradecanoate-decahydrate. The magnesium hydroxide is placed in a covered alumina crucible, 11 〇〇 〇 〇 〇 大气 大气 大气 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 〇 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气 大气The diameter is 1.68 " m, the median diameter is obtained from the particle size distribution.... The specific surface area diameter calculated from the specific surface area is 16..., and the median diameter is obtained from the particle size distribution. The specific surface area diameter is 2_60 〇 and 'D90 is 6.79 ν m, D10 Α ^ μ m is 1.75 β m > The value of D9〇/DIO was 3.88. (Example 2) Magnesium oxide particles-b The same operation as in Example 1 was carried out except that the amount of sodium sulphate-decahydrate was 8.20 g. Particle 4. The amount of sodium tetraborate--hydrate added at this time is converted to 〇·5 mol by the amount of 曾 Λ 乂 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM SEM ; , , ',,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, The value of the specific diameter of the seven + +, orthodontic knife is 丨y, and the D90 is 6.22 μm. The value of Dl〇 is 2.35. The value of D9〇/Dl〇 is 2 65.
C (實施例3)氧化鎂粒子 201111282 除了代替四硼酸鈉—μ 士人1 α 卞水合物，將四硼酸鐘一五水合 物設為5·57 g以外’進行與實施例ι相同之操作，獲得氧 ，錢粒子1。此時添加之四爛酸鐘_五水合物之量以石朋換 算為0.5 mol份。由該氧仆招加7 , 羊匕化鎂粒子一c之S EM照片求得之一 次粒徑為2.1 1 " m，由妹立许八任. m !刀佈求得之中徑為4.28 // m， 由比表面積算出之比表面積彳, 叫預彳工马2.02 μ m，由粒度分佈求 得之中徑/由比表面穑灰锃 尺仔之比表面積徑之值為2.03。又， D90 為 6.75 /zm，Dl〇A 9 马 2.56 // m，D90/D10 之值為 2.64。 (實施例4)氧化鎂粒子—d 除了代替四棚酸麵__I I，Λ ^ 十水合物，將四硼酸鉀一四水合 物-又為6.57 g以外’進行與實施例"目同之操作，獲得氧 ，鎮粒子-d。此時添加之明酸鉀—四水合物之量以石朋換 算為0.5 mo 1份。由該最卟铝如7 , 乳化鎂拉子—d之SEM照片求得之一 次粒徑為2 _ 16 # m，由知*八+上、 l , M 由拉度分佈求得之中徑為4.34 A m， 由比表面積算出之比表面積徑為2〇6 "m，由粒度分佈求 得之中徑/由比表面積求得之比表面積徑之值為2.01。又， D90 為 6_65 ym、Dl〇 為^ ^, Λ 馬.48 " m’D90/D10 之值為 2 68。 (實施例5)氧化鎮粒子__ e 除了代替四爛酸納—十水合物，將四蝴酸錢_四水合 物:又為5.66g以外，進行與實施例i相同之操作獲得氧化 鎂粒子-e 〇此時添加之四硼酸銨一四水合物之量以硼換算 為0.5爪〇1份。由該氧化鎂粒子—e之seM照片求得之一次 粒徑為2_16㈣，由粒度分佈求得之中徑為（34…由 比表面積算出之比表面穑僻& ^ 檟k為2.06 gm，由粒度分佈求得 20 201111282 之中徑/由比表面積求得之卜 <比表面積徑之值為2 D90 為 6.65 " m，D10 為 2 ,, 勺（48 y m，D9〇/m〇 之 1 (實施例6)氧化鎂粒子__ f 除了將四職-十水合物之量設為82 0 g 行與糊1相同之操作，獲得氧化鎮粒子—f。 之四删酸納—十水合物之量以爛換算為5 mol份。 鎂粒子-f之SEM"求得之—次粒徑為a / 度：佈求得之中徑為4.02…由比表面積算出 積徑為2.3 1 # m，由粒度分佈求得之中徑/由比 得之比表面積徑之值為丨.74。又，D90為6 53 為 2.48 // m ’ D90/D10 之值為 2 63。 (實施例7)氧化鎂粒子—g 除了將四硼酸鈉一十水合物之量設為丨3丨2 @ 行與實施例1相同之操作，獲得氧化鎂粒子—g。 之四硼酸鈉一十水合物之量以硼換算為8 m〇l份。 鐄粒子一 g之SEM照片求得之一次粒徑為2 3 9 ^ 度分佈求抑之中徑為4.58 ym，由比表面積算出 積徑為2.46 y m，由粒度分佈求得之令徑/由比 得之比表面積徑之值為1.86。又，D90為6.86 為 2.56 # m，D90/D10 之值為 2.68。 (實施例8)氧化鎂粒子_ h 除了將四硼酸鈉一十水合物之量設為16 4 g、 設為1000°C以外，進行與實施例1相同之操作， 鱗粒子_ h。此時添加之四棚酸納--卜水合物之量 _〇1 〇 又， 良為2.68。 以外，進 此時添加 由該氧化 ^ m，由粗 之比表面 ‘表面積求 U m > Dl〇 :以外，進 此時添加 由該氧化 i m，由粒 之比表面 表面積求 U m > Dl〇 煅燒溫度 獲得氧化 以硼換算 21 201111282 為1副份。由該氧化鎮粒子—^咖照片求得之一次 粒徑為1…m ’由粒度分佈求得之中徑為4.43 "m，由 比表面積算出之比表面積徑為丨5〇 "爪，由粒度分佈求得 之中徑/由比表面積求得之比表面積徑之值為2.95。又， 〇90為6.62以1!1，〇1〇111^： , 〇 為！·76 " m，D90/D10 之值為 3 76。 (實施例9)氧化鎂粒子 …除了將四石朋酸鈉—十水合物之量設$ 16.4§、般燒溫度 叹為1200 C^卜’進行與實施例丨相^之操作獲得氧化 鎮粒子1。此時添加之四刪酸納—十水合物之量以侧換算 為1 mol份。由該氧化鎂粒子—SEM照片求得之一次粒 徑為3.14 vm，由粒度分佈求得之中徑為6 58 “⑺，由比 表面積算出之比表面積徑為328 ，由粒度分佈求得之 中fe/由比表面積求得之比表面積徑之值為2 gi。又謂 為 8.12 //m，Dl〇 為 3.56 #m，D9()/D1()之值為 U (實施例10)氧化鎂粒子一』 除了將四硼酸鈉—十水合物之量設為16.4 g、煅燒溫度 设為1400 C以外，進行與實施例i相同之操作，獲得氧化 鎂粒子一 j。此時添加之四硼酸鈉—十水合物之量以硼換曾 為1 mol份。由該氧化鎂粒子—j之SEM照片求得之一次粒 杻為8.61 " m，由粒度分佈求得之中徑為19 2以爪，由比 表面積算出之比表面積徑為9. 〇丨# m，由粒度分佈求得之 中徑/由比表面積求得之比表面積徑之值為2.13。又，D卯 為 25.3 //m，Dl〇g119 #m，D90/D10 之值為 212。 (實施例1 1)氧化鎂粒子一 k 22 201111282 除了將四硼酸鈉一十水合物之量設為1 64 g、煅燒溫度 設為1600°C以外，進行與實施例1相同之操作，獲得氧化 鎮粒子一k。此時添加之四硼酸鈉一十水合物之量以删換算 為1 m ο 1份。由5亥氧化鎮粒子—k之§ £ μ照片求得之_ A 粒徑為12.1 #m，由粒度分佈求得之中徑為23 $以爪，由 比表面積算出之比表面積徑為13.〇 μιη，由粒度分佈求得 之中徑/由比表面積求得之比表面積徑之值為18丨。又， D90 為 29.8 #m，Dl〇 為 18_2 "m，D9〇/Dl〇 之值為！— (實施例12)氧化鎂粒子一 1 將實施例2獲得之氧化鎂 © 1 >Γ々月又王甲醇 (和光純藥）100 ml中，加入乙酸（和光純藥）〇 〇2 g、癸基三 甲氧基石夕⑥（KBM-3103C;信越化學）！ g，於搜掉下加入純 水1 g’㈣1小時後，進行過據、乾燥、粉碎而獲得氧化 錢粒子-1。將該氧化鎂粒子一 ！放入溫度85〇c、濕度85% 之恒溫恒濕器中，觀察重量變化，結果經㉟5⑻小時 觀察到質量增加。 (比較例1)氧化鎂粒子—m 除了將四魏納—十水合物之量設為Q.82g、炮燒溫度 设為moc以外，進行與實施例i相同之操作，獲得氧化 鎮粒子-m。此時添加之明酸納_十水合物之量以蝴換算 為0.0 5 πί ο 1份。由該氧/卜姓士 7 田及氧化鎂粒子—爪之SEM照片求得之一 次粒徑為0.98心，由粒度分佈求得之中徑為以 由比表面積算出之比表面積徑為1G5㈣，由粒度分佈求 付之中徑/由比表面積求得之比表面積徑之值為3.10。又， 23 201111282 D90 為 6.21 " m，DU)為 us M m’D9〇/Dl〇 之值為 * 5〇 (比較例2)氡化鎂粒子一 ^ 除了不添加四硼酸鈉—十水合物、將煅燒溫度設為 1 200°C以外，進行與實施例 子一η。由該氧化鎂粒子—η 1相同之操作，獲得氧化鎂粒 之SEM照片求得之一次粒徑為 0.76 Mm，由粒度分佈求得之中徑為3 〇2从爪，由比表面 積算出之比表面積徑為〇.79 M m ’由粒度分佈求得之中徑 /由比表面積求得之比表面積徑之值為3 82。又，D卯為 5·88 //m’DIO ^，謂/叫之值為（μ。 (實施例13〜24) 以表1所示之比例將EEA樹脂（A— U5〇日本聚乙烯公 司製）及實施例1〜12之氧化鎂粒子加熱至16〇它，同時進 行混合，其後藉由加壓成形獲得樹脂成型體。將其製成直 徑50 mmx厚度2 mm之形狀之成型體。測定該等之導熱率。 再者，導熱率係藉由熱流計法於25<>c進行測定。 (實施例25) 以表1所示之比例將EEA樹脂（A— 1150 13本聚乙烯公 司製)及實施例8與實施例"之氧化鎂粒子加熱至16〇。。， 同時進打混合’其後藉由加壓成形獲得樹脂成型體。將其 製成直徑50 mmx厚度2 _之形狀之成型體。測定該等^ 導熱率。再者’導熱率係藉由熱流計法於坑進行測定。 (實施例26) 於以表1所不之比例將EEA樹脂（A — 1丨5〇曰本聚乙烯 公司製)及實施例8與實施例"之氧化鎂粒子混合而成者中 24 201111282 進而加入得化学工業製氧化鎮（S EM徑〇. 1 v m)，加熱至 1 60。(：之同時進行混合’其後藉由加壓成形獲得樹脂成型 體。將其製成直徑50 mmx厚度2 mm之形狀之成型體。測 定該等之導熱率。再者’導熱率係藉由熱流計法於25。(：進 行測定。 (比較例3) 除了不摻合氧化鎮粒子以外’與實施例1 3同樣地測定 導熱率。結果示於表1。 (比較例4〜6) 除了使用氧化鋁代替氧化鎂粒子以外，與實施例13同 樣地測定導熱率。結果示於表1。 25 201111282 Ο m m 比較例 CN 00 o v〇 00 in r-； 寸 (N ^Τ) 00 Ό VO od in (N rs 實施例 (N 〇 Os — CN r^ ro r^ ON rvi \〇 00 ro (N o 00 卜 1-*^ 寸 〇\ \〇 Ό rn 艺 o r*-* ί〇 cK iri 〇\ Ό (N ΓΛ CN o ΚΤ) cK Os v〇 v〇 r〇 (N (N o in cK v〇 ro CN o f—^ cK a\ r^i Ό 对 ro o iri On Os rsi ^o 卜 <N 〇\ o ΙΤϊ cK u-> On v〇 rn 00 o V) cK *T) 〇\ m ro 卜 o ίη On m σ> rsi Ό ro VO o ίΛ> cK On v〇 ΓΛ r'i o ON σν CM· Ό 寸 o ITi 〇\ Ό cn γ^Ί ΓΛ o 〇\ r^i 00 oi 比較例 ro o o ΓΊ d EEA樹脂 cd x> o T3 <υ W) X： •»— ·—> — 堺化學工業製氧化鎂 (SEM 徑 0.1 "m) 氧化銘20 "m 氧化铭10 "m 氧化铭0.8 //m 填料(體積％) 導熱率(\V/nvK) 聲φ_(桃_拿） 201111282 (實施例27) 以表2所示之比例混合環氧樹脂（jERg28 Japan Epoxy Resins公司製）、環氧樹脂硬化劑（jERCURE ST12 Japan Epoxy Resins公司製）及實施例ι〇之氧化鎂粒子—j，注入 至直徑50 mmx高度2 mm之模具中，藉由於8〇°C熱處理3 小時而獲得成型體。將測定該成型體之導熱率之結果示於 表2。 (比較例7) 除了氧化鎂粒子一j以外’亦使用氧化鋁丨〇 μ m，除 此以外與實施例27同樣地測定導熱率。結果示於表2。 [表2] 質摻 量合 份量 實施例27 比較例7 環氡樹脂 12 12 環氧樹脂硬化劑 6 6 實施例10之氧化鎂 17.4 氧化紹10 "m 20 填料(體積％) 25 25 導熱率(W/nrK) 0.6 0.3 (實施例28) 以表3所示之比例，混合矽樹脂（KE _丨〇3信越化學工 業公司製）、矽樹脂硬化劑（CAT ~ 1 〇3信越化學工業公司製） 及實施例10之氧化鎂粒子_ j，加熱至]5，同時加壓成 形30分鐘，藉此獲得樹脂組成物。將其製成直徑5〇 mmx 厚2 mm之形狀之成型體，將測定導熱率之結果示於表3。 (比較例8) 27 201111282 除了氧化鎂粒子一i以外，亦使用氧化鋁〗〇以出，除 此以外與實施例28同樣地測定導熱率。結果示於表3。。 [表3] f摻 量合 份量 實施例28 比較例8 石夕樹脂 14 14 妙樹脂硬化杳1丨 0.7 0.7 實施例10之氣化锃 52.1 氧化紹10 // m 60 填料(體積。/〇) 50 50 導熱率(W/nrK) 2.1 1.4 (實施例29) 藉由以表4所示之比例，混合矽油（KF — 99信越化學工 業公司製）、及實施例1 0之氧化鎂粒子一」而製作散熱性潤 滑脂。將測定該散熱性潤滑脂之導熱率之結果示於表4。 (比較例9) 除了氧化鎂粒子一 j以外’亦使用氧化鋁1〇 V m，除 此以外與實施例29同樣地測定導熱率。結果示於表4。 [表4] f # 量合 份量 實施例29 比較例9 矽油 5 5 實施例10之氧化鎂 17.4 氧化铭10 20 填料(體積％) 50 50 導熱率(W/m-K) 1.8 1.2 (實施例30) 藉由以表5所示之比例，利用分散機分散環氧樹脂 28 201111282 (jER828 Japan Epoxy Resins公司製）、曱苯及實施例l〇之 氧化鎂粒子一 j而製作散熱性塗料。將測定該散熱性塗料組 成物之導熱率之結果示於表5。 (比較例10) 除了氧化鎂粒子一 j以外，亦使用氧化鋁1 〇 μ m，除 此以外與實施例30同樣地測定導熱率。結果示於表5。 [表5] f摻 4合 份量 'W 實施例30 比較例10 環氧樹脂 6.3 6.3 曱苯 11.7 11.7 實施例10之氧化鎂 34.7 氧化is 10 " m 40 填料(體積％) 35 35 導熱率(W/nrK) 1.4 0.9 田衣1〜5之結果可明確，本發明之散熱性填料係具 比廣泛使用之散熱性填料更優異之性能者。又明確二 摻合〜尚摻合之任一情況下均可賦予散熱性。 ^ *·座苐上之可利用性] 本發明之氧化鎮粒子可較佳地用作散熱性填料， 外亦可用於橡膠之硫化促進n 藥品等用途。 額科，醫 【圖式簡單說明】 M.C (Example 3) Magnesium oxide particles 201111282 The same operation as in Example ι was carried out except that sodium tetraborate-μs human 1 α hydrazine hydrate was used, and tetraboric acid penta pentahydrate was set to be 5.57 g. Obtain oxygen, money particles 1. At this time, the amount of the four rotten acid clock _pentahydrate added was changed to 0.5 mol by Shi Peng. From the oxygen servant, 7 , the S EM photo of the magnesium granules of the yttrium sulphate, the primary particle size is 2.1 1 " m, by the sister Li Xu ren. m ! knife cloth to obtain a medium diameter of 4.28 // m, the specific surface area 彳 calculated from the specific surface area is called 2.02 μm of the pre-worker horse, and the median diameter from the particle size distribution/the specific surface area diameter of the specific surface ash is 2.03. Also, D90 is 6.75 /zm, Dl〇A 9 is 2.56 // m, and D90/D10 is 2.64. (Example 4) Magnesium oxide particles - d In addition to replacing the tetrakis acid surface __I I, Λ ^ decahydrate, potassium tetraborate monohydrate - again 6.57 g 'together with the embodiment' Operation, obtaining oxygen, town particles - d. The amount of potassium citrate-tetrahydrate added at this time was changed to 0.5 mol 1 part by Shi Peng. The primary particle diameter obtained from the SEM photograph of the most bismuth aluminum such as 7 and the emulsified magnesium puller-d is 2 _ 16 # m, and the median diameter is obtained from the distribution of the *8+up, l, M 4.34 A m , the specific surface area diameter calculated from the specific surface area is 2〇6 "m, and the median diameter obtained from the particle size distribution/the specific surface area diameter obtained from the specific surface area is 2.01. Also, D90 is 6_65 ym, Dl〇 is ^^, and Λ马.48 " m'D90/D10 has a value of 2 68. (Example 5) Oxidation of the granules __ e In the same manner as in Example i except that instead of the tetrahydronate sodium-decahydrate, the same operation as in Example i was carried out, except that the tetracabic acid _tetrahydrate: 5.66 g was obtained. -e 〇 The amount of ammonium tetraborate monohydrate added at this time is 0.5 part by weight in terms of boron. The primary particle diameter obtained from the seM photo of the magnesium oxide particle-e is 2_16 (four), and the median diameter is obtained from the particle size distribution (34...the specific surface area calculated from the specific surface area is & ^ 槚k is 2.06 gm, by particle size The distribution obtained 20 201111282 medium diameter / obtained by the specific surface area < specific surface area diameter of 2 D90 is 6.65 " m, D10 is 2, spoon (48 ym, D9〇 / m〇 1 (implementation Example 6) Magnesium Oxide Particles __ f In addition to the operation of the amount of the tetra-decahydrate to 82 0 g, the same operation as the paste 1 was carried out to obtain the amount of the oxidized town particle-f. In terms of rotten, it is converted into 5 mol parts. The SEM of the magnesium particles-f is obtained. The sub-particle size is a / degree: the medium diameter is 4.02... The specific diameter is calculated from the specific surface area of 2.3 1 # m, by the particle size distribution. The diameter of the specific diameter of the intermediate diameter/comparison is 丨.74. Further, D90 is 6 53 for 2.48 // m ' D90/D10 is 2 63. (Example 7) Magnesium oxide particles-g The sodium tetraborate monohydrate was obtained by the same operation as in Example 1 except that the amount of sodium tetraborate monohydrate was set to 丨3丨2 @. The amount is 8 m〇l in terms of boron. The SEM image of the 鐄 particle-g is a primary particle size of 2 3 9 ^ degree distribution with a median diameter of 4.58 ym, and the calculated specific surface area is 2.46 ym. The particle size distribution obtained by the diameter/ratio of the specific surface area diameter is 1.86. Further, D90 is 6.86 to 2.56 #m, and the value of D90/D10 is 2.68. (Example 8) Magnesium oxide particles _ h In addition to four The amount of sodium borate-decahydrate was set to 16 4 g, and it was set to 1000 ° C, and the same operation as in Example 1 was carried out, and the scale particles _ h. The amount of sodium sulfonate-buhydrate added at this time _〇1 〇 again, good is 2.68. In addition, at this time, the addition of the oxidation ^ m, from the surface ratio of the surface of the rough surface, U m > Dl〇: The ratio of surface area to U m > Dl 〇 calcination temperature to obtain oxidation in terms of boron conversion 21 201111282 is 1 part. The primary particle size obtained from the oxidized town particle - ^ coffee photo is 1...m 'from the particle size distribution The median diameter is 4.43 "m, and the specific surface area calculated from the specific surface area is 丨5〇"claw, which is determined by the particle size distribution. The median diameter/the specific surface area diameter determined by the specific surface area is 2.95. Further, 〇90 is 6.62 to 1!1, 〇1〇111^: , 〇 is !·76 " m, the value of D90/D10 is 3 76. (Example 9) Magnesium oxide particles... In addition to the amount of sodium tetrasphenate-decahydrate, the amount of sulphur-containing granules was set at 1200 C^b. 1. The amount of the tetradecanoate-decahydrate added at this time was 1 mol part by side. The primary particle diameter obtained from the SEM photograph of the magnesium oxide particles was 3.14 vm, and the median diameter was 6 58 "(7), and the specific surface area calculated from the specific surface area was 328, which was obtained from the particle size distribution. / The specific surface area diameter determined by the specific surface area is 2 gi. Also known as 8.12 //m, Dl〇 is 3.56 #m, and the value of D9()/D1() is U (Example 10) Magnesium oxide particles In the same manner as in Example i except that the amount of sodium tetraborate-decahydrate was 16.4 g and the calcination temperature was 1400 C, magnesium oxide particles were obtained in the same manner. The amount of hydrate was changed to 1 mol by boron. The primary granule obtained from the SEM photograph of the magnesium oxide particle-j was 8.61 " m, and the median diameter was 19 2 to obtain the claw, the ratio The specific surface area diameter calculated by the surface area is 9. 〇丨# m, and the median diameter obtained from the particle size distribution/the specific surface area diameter determined by the specific surface area is 2.13. Further, D卯 is 25.3 //m, Dl〇g119 # m, D90/D10 has a value of 212. (Example 1 1) Magnesium oxide particles-k 22 201111282 In addition to sodium tetraborate decahydrate The amount was set to 1 64 g, and the calcination temperature was set to 1600 ° C. The same operation as in Example 1 was carried out to obtain oxidized particles - k. The amount of sodium tetraborate monohydrate added at this time was converted into 1 m ο 1 part. From the 5 oxidized town particle - k § £ μ photo obtained _ A particle size is 12.1 #m, the median diameter is 23 $ to obtain the claw, the ratio calculated from the specific surface area The surface area diameter is 13. 〇μιη, and the median diameter obtained from the particle size distribution/the specific surface area diameter determined by the specific surface area is 18 丨. Further, D90 is 29.8 #m, Dl〇 is 18_2 "m, D9〇/ The value of Dl〇 is - (Example 12) Magnesium oxide particles - 1 The magnesium oxide obtained in Example 2 is added to acetic acid (Wako Pure Chemical Co., Ltd.) 〇〇2 g, fluorenyltrimethoxy sinus 6 (KBM-3103C; Shin-Etsu Chemical)! g, after adding 1 g of water (1) for 1 hour after searching, it was dried, pulverized to obtain oxidized money particles. -1. The magnesium oxide particles were placed in a thermo-hygrostat having a temperature of 85 ° C and a humidity of 85%, and the weight change was observed. The mass increase was observed at 5 (8) hours. (Comparative Example 1) Magnesium oxide particles - m The same operation as in Example i was carried out except that the amount of the tetrawei-decahydrate was Q.82 g and the calcination temperature was set to moc. The oxidized town particle-m is obtained. The amount of sodium decoxide added to the hydrate is 0.0 5 π ί ο 1 part. The primary particle diameter obtained from the SEM photograph of the oxygen/Bus 7 field and the magnesium oxide particles-claw is 0.98 core, and the median diameter determined by the particle size distribution is the specific surface area calculated from the specific surface area, and the specific surface diameter is 1 G5 (four). The distribution of the median diameter/the specific surface area obtained from the specific surface area has a value of 3.10. Further, 23 201111282 D90 is 6.21 " m, DU) is the value of us M m'D9〇/Dl〇* 5〇 (Comparative Example 2) Magnesium telluride particles ^ except that sodium tetraborate-decahydrate is not added Further, the calcination temperature was set to 1 200 ° C, and η was carried out in the same manner as in Example 1. From the same operation of the magnesium oxide particles - η 1 , the primary particle diameter obtained by obtaining the SEM photograph of the magnesium oxide particles was 0.76 Mm, and the median diameter was 3 〇 2 from the claw, and the specific surface area was calculated from the specific surface area. The diameter is 〇.79 M m 'The median diameter obtained from the particle size distribution/the specific surface area diameter obtained from the specific surface area is 3 82 . Further, D卯 is 5.88 //m'DIO ^, and the value is called (μ. (Examples 13 to 24) EEA resin (A-U5〇 Japan Polyethylene Co., Ltd.) is shown in the ratio shown in Table 1. The magnesium oxide particles of the examples 1 to 12 were heated to 16 Torr while being mixed, and then a resin molded body was obtained by press molding, and this was molded into a molded body having a diameter of 50 mm x a thickness of 2 mm. The thermal conductivity was measured. Further, the thermal conductivity was measured by a heat flow method at 25 ° C. (Example 25) EEA resin (A-1150 13 polyethylene) was used in the ratio shown in Table 1. The company and the embodiment 3 and the magnesium oxide particles of the embodiment " were heated to 16 〇., while mixing and mixing', and then the resin molded body was obtained by press molding. It was made into a diameter of 50 mm x thickness 2 _ The molded body of the shape was measured for the thermal conductivity. Further, the thermal conductivity was measured by a heat flow method in a pit. (Example 26) EEA resin (A-1 丨) was used in a ratio not shown in Table 1. 5 〇曰 聚乙烯 聚乙烯 聚乙烯 及 及 及 聚乙烯 聚乙烯 聚乙烯 聚乙烯 聚乙烯 聚乙烯 24 24 24 24 24 24 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 2011 Industrial oxidized town (S EM diameter 1 1 vm), heated to 1600. (: Simultaneous mixing is carried out) Thereafter, a resin molded body is obtained by press forming. It is made into a diameter of 50 mm x a thickness of 2 mm. Shaped molded body. The thermal conductivity of these was measured. Further, the thermal conductivity was measured by a heat flow method at 25. (: Comparative Example 3) (Comparative Example 3) Except that the oxidized granules were not blended, and Example 1 3 The thermal conductivity was measured in the same manner. The results are shown in Table 1. (Comparative Examples 4 to 6) The thermal conductivity was measured in the same manner as in Example 13 except that alumina was used instead of the magnesium oxide particles. The results are shown in Table 1. 25 201111282 Ο mm Comparison Example CN 00 ov〇00 in r-; inch (N ^Τ) 00 Ό VO od in (N rs embodiment (N 〇Os — CN r^ ro r^ ON rvi \〇00 ro (N o 00 卜 1- *^ inch〇\ \〇Ό rn art or*-* 〇〇cK iri 〇\ Ό (N ΓΛ CN o ΚΤ) cK Os v〇v〇r〇(N (N o in cK v〇ro CN of-^ cK a\ r^i Ό for ro o iri On Os rsi ^o 卜<N 〇\ o ΙΤϊ cK u-> On v〇rn 00 o V) cK *T) 〇\ m ro 卜o ίη On m σ> rsi Ό ro VO o ίΛ> cK On V〇ΓΛ r'i o ON σν CM· Ό inch o ITi 〇\ Ό cn γ^Ί ΓΛ o 〇\ r^i 00 oi Comparative example ro oo ΓΊ d EEA resin cd x> o T3 <υ W) X : •»————> — Magnesium oxide produced by 堺Chemical Industry (SEM diameter 0.1 "m) Oxidation Ming 20 "m Oxidation Ming 10 "m Oxidation Ming 0.8 //m Filler (% by volume) Thermal conductivity (\ V/nvK) Sound φ_(桃_拿) 201111282 (Example 27) Epoxy resin (jERg28 Japan Epoxy Resins Co., Ltd.) and epoxy resin hardener (jERCURE ST12 Japan Epoxy Resins Co., Ltd.) were mixed at a ratio shown in Table 2. And the magnesium oxide particles-j of the example 〇 were injected into a mold having a diameter of 50 mm x a height of 2 mm, and a molded body was obtained by heat treatment at 8 ° C for 3 hours. The results of measuring the thermal conductivity of the molded body are shown in Table 2. (Comparative Example 7) The thermal conductivity was measured in the same manner as in Example 27 except that the alumina 丨〇 μ m was used in addition to the magnesium oxide particles. The results are shown in Table 2. [Table 2] Amount of the compounded amount of Example 27 Comparative Example 7 Cyclodecyl resin 12 12 Epoxy resin hardener 6 6 Magnesium oxide of Example 10 17.4 Oxidation 10 "m 20 Filler (% by volume) 25 25 Thermal conductivity (W/nrK) 0.6 0.3 (Example 28) In the ratio shown in Table 3, an anthracene resin (KE _丨〇3, Shin-Etsu Chemical Co., Ltd.), an epoxy resin hardener (CAT ~ 1 〇3 Shin-Etsu Chemical Co., Ltd.) was mixed. The magnesium oxide particles _ j of Example 10 were heated to 5 while being press-formed for 30 minutes, whereby a resin composition was obtained. The molded body having a shape of a diameter of 5 mm mm and a thickness of 2 mm was used, and the results of measuring the thermal conductivity are shown in Table 3. (Comparative Example 8) 27 201111282 The thermal conductivity was measured in the same manner as in Example 28 except that the alumina particles were used in the same manner as in the case of the magnesium oxide particles. The results are shown in Table 3. . [Table 3] f blending amount of Example 28 Comparative Example 8 Shixi Resin 14 14 Resin Hardened 杳1丨0.7 0.7 Vaporized hydrazine of Example 10 52.1 Oxidation 10 // m 60 Filler (volume./〇) 50 50 Thermal conductivity (W/nrK) 2.1 1.4 (Example 29) By mixing the eucalyptus oil (KF-99 Shin-Etsu Chemical Co., Ltd.) and the magnesium oxide particles of Example 10 by the ratio shown in Table 4 And make a heat-dissipating grease. The results of measuring the thermal conductivity of the heat-dissipating grease are shown in Table 4. (Comparative Example 9) The thermal conductivity was measured in the same manner as in Example 29 except that the alumina 1 〇 V m was used in addition to the magnesium oxide particles. The results are shown in Table 4. [Table 4] f # Quantities Part 29 Comparative Example 9 Emu Oil 5 5 Magnesium Oxide of Example 10 17.4 Oxidation Ming 10 20 Filler (% by volume) 50 50 Thermal conductivity (W/mK) 1.8 1.2 (Example 30) A heat-dissipating paint was prepared by dispersing epoxy resin 28 201111282 (manufactured by jER828 Japan Epoxy Resins Co., Ltd.), benzene, and magnesium oxide particles of Example 1 by a disperser at a ratio shown in Table 5. The results of measuring the thermal conductivity of the heat-dissipating paint composition are shown in Table 5. (Comparative Example 10) The thermal conductivity was measured in the same manner as in Example 30 except that the alumina particles were used in addition to the magnesium oxide particles. The results are shown in Table 5. [Table 5] f in 4 parts by weight 'W Example 30 Comparative Example 10 Epoxy Resin 6.3 6.3 Toluene 11.7 11.7 Magnesium Oxide of Example 10 34.7 Oxidation is 10 " m 40 Filler (% by volume) 35 35 Thermal conductivity ( W/nrK) 1.4 0.9 As a result of the field clothing 1 to 5, it is clear that the heat-dissipating filler of the present invention has superior performance to the widely used heat-dissipating filler. It is also clear that the heat dissipation can be imparted in any of the two blends to the blending. ^ *· Usability in the seat] The oxidized particles of the present invention can be preferably used as a heat-releasing filler, and can also be used for vulcanization of rubber to promote n-drugs and the like. Forehead, medical [simplified illustration] M.
t ON 【主要元件符號說明】 益 ***、 29t ON [Key component symbol description] Benefit ***, 29